Timo Paakkari

Crystallinity of wood and the size of cellulose crystallites in Norway spruce (Picea abies)

X-ray diffraction was used to study variations in the crystallinity of wood and the average thickness and length of the crystallites of cellulose as a function of the number of the year ring in Norway spruce [Picea abies (L.) Karst.]. The crystallinity increased from ring 4 to ring 10 from the pith and was constant after ring 10. The crystallinity of mature wood was about 30% ± 5%. The average thickness and average length of the crystallites were 3.2 ± 0.1 nm and 28 ± 2 nm, respectively; and no systematic variation of these values with the number of the year ring was observed. The mean microfibril angle decreased near the pith but was constant in the mature wood.

Novel Identification of Pseudopolymorphic Changes of Theophylline During Wet Granulation Using Near Infrared Spectroscopy

The purpose of this study was to demonstrate the efficiency of near infrared (NIR) spectroscopy in studying the pseudopolymorphic changes and the state of water during the wet granulation process. Anhydrous theophylline was granulated in a planetary mixer using water as granulation liquid. NIR spectra and differential scanning calorimetric (DSC) and wide-angle X-ray scattering (WAXS) patterns of theophylline granules, anhydrous theophylline, and theophylline monohydrate were measured. At a low level of granulation liquid (0.3 mol of water per mole of anhydrous theophylline), water absorption maxima in the NIR region occurred first at around 1475 and 1970 nm. These absorption maxima were identical to those of theophylline monohydrate. At higher levels of granulation liquid (1.3-2.7 mol of water per mole of anhydrous theophylline), the increasing absorption maxima occurred at 1410 and 1905 nm due to OH vibrations of free water molecules. X-ray diffraction patterns confirmed the transformation of anhydrous theophylline to theophylline monohydrate during wet granulation. NIR spectroscopy was able to detect different states of water molecules during the wet granulation process faster and in a more flexible manner than conventional methods.

Microfibril angle of Norway spruce [Picea abies (L.) Karst.] compression wood: comparison of measuring techniques.

The structure of cellulose, especially the microfibril angles (MFAs), in compression wood of Norway spruce [Picea abies (L.) Karst.] was studied by wide- and small-angle X-ray scattering and polarizing microscopy. On the basis of the X-ray scattering experiments the average MF As of the cell wall layers S2 and S1 of the studied sample are 39‡ and 89‡, respectively; and the average diameter and length of the cellulose crystallites are 2.9 and 20.0nm, respectively. The average of the whole MFA distribution is shown to agree with the one obtained by polarizing microscopy of macerated fibers.

X-ray scattering studies of thermally modified Scots pine (Pinus sylvestris L.)

Abstract Wood is thermally modified by heating and steaming in order to change its properties, e.g., to improve the biological resistance and to increase the hardness of wood. The structure of thermally modified Scots pine (Pinus sylvestris) was studied using wide-angle, small-angle and ultra-small-angle X-ray scattering methods. Modification temperatures varied from 100 to 240°C. No marked changes in the microfibril angle distribution were observed. The mass fraction of crystalline cellulose in wood (the crystallinity of wood) and the size of cellulose crystallites increased above 150°C. After modification at 230°C for 4 h the thickness of the cellulose crystallites increased from 3.1 to 3.4 nm. Thermal modification had no effect on the orientation of the voids, but an increase in the porosity of the cell wall was observed. The distance between cellulose crystallites was approximately 4.7 nm in hydrated wood and a decrease in order between microfibrils was observed at 160–200°C.

The structure of amorphous cellulose as revealed by wide-angle X-ray scattering

Abstract The structure of amorphized cellulose samples prepared by ball milling of cellulose I and II and by saponification of cellulose triacetate is investigated by means of radial distribution functions (RDFs). Experimental wide-angle X-ray scattering results are compared with model calculations assuming atomic positions arising from different crystal structure investigations. At small atomic distances ( r r > 0.5 nm larger differences exist between experimental and model RDFs, indicating increased distances as compared with the crystalline state.

The elemental composition, the microfibril angle distribution and the shape of the cell cross-section in Norway spruce xylem

Relationships between the elemental composition, the microfibril angle (MFA) distribution and the average shape of the cell cross-section of irrigated-fertilised and untreated Norway spruce (Picea abies [L.] Karst.) earlywood were studied. Sample material was obtained from Flakaliden, Sweden. The elemental composition was studied by determining the relative mass fractions of the elements P, S, Cl, K, Ca and Mn by X-ray fluorescence and by determining the mass absorption coefficients for X-rays. X-ray diffraction was used to determine the MFA distribution and the average shape of the cell cross-section. The latter was also determined by light microscopy. In transition from juvenile wood to mature wood, a decrease of the mode of the MFA distribution from 13°–24° to 3°–6° was connected to a change in the shape of the cell cross-section from circular to rectangular. The irrigation-fertilisation treatment caused no change in the MFA distribution or in the shape of the cell cross-section, whereas the mass absorption coefficient was higher and the density was smaller in irrigated-fertilised wood. Larger proportion of the elements S, Cl and K, but smaller proportion of the element Mn, were observed due to the treatment. The results indicate that the shape of the cell cross-section or the MFA distribution are not directly linked to the growth rate of tracheids or to the nutrient-element content in the xylem and only show notable changes as a function of the cambial age.

Aggregation of platinum-uridine blue as a function of concentration in aqueous solution by small angle X-ray scattering

Abstract Aqueous solutions of amorphous platinum-uridine blue were studied by the small angle X-ray scattering method in the concentration range 1.4–140 mg/ml. The results showed a dependence on concentration, which was interpreted with the aid of computer simulations as arising from aggregation of dinuclear Pt units. The radii of gyration of the aggregates varied between 6 and 15 A.